CN110668503A - Double-layer perovskite manganese oxide single-phase thin film material with vertically arranged nano structure and preparation method thereof - Google Patents

Double-layer perovskite manganese oxide single-phase thin film material with vertically arranged nano structure and preparation method thereof Download PDF

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CN110668503A
CN110668503A CN201910920569.2A CN201910920569A CN110668503A CN 110668503 A CN110668503 A CN 110668503A CN 201910920569 A CN201910920569 A CN 201910920569A CN 110668503 A CN110668503 A CN 110668503A
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manganese oxide
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CN110668503B (en
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张科军
刘剑敏
戴建明
朱雪斌
孙玉平
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Jingchu University of Technology
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    • C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
    • C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
    • C01G45/1264—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3 containing rare earth, e.g. La1-xCaxMnO3, LaMnO3
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Abstract

The invention discloses a double-layer perovskite manganese oxide single-phase thin film material with a vertically arranged nano structure, which is grown on a substrate, and the chemical formula of the double-layer perovskite manganese oxide single-phase thin film material is La1‑xCaxMnO3X is more than 0.35 and less than or equal to 1, the double-layer structure of the nano-structure comprises a continuous layer with the thickness of 0-40 nm and epitaxially grown along the substrate and a nano-column layer vertical to the continuous layer, and the nano-column layer epitaxially grows along the continuous layer. The invention also discloses a double-layer calcium with vertically arranged nano-structuresA preparation method and application of a single-phase titanium ore manganese oxide film material. The material of the invention has obvious perpendicular magnetic anisotropy and adjustable low-field magnetoresistance effect with wide working temperature range.

Description

Double-layer perovskite manganese oxide single-phase thin film material with vertically arranged nano structure and preparation method thereof
Technical Field
The invention relates to the field of manganese oxide thin film materials, in particular to a double-layer perovskite manganese oxide single-phase thin film material with a vertically arranged nano structure and a preparation method thereof.
Background
The complex oxide thin film material with vertically aligned nano-structures is significantly different from the conventional planar film structure in characteristics and functionality because it has a vertical interface area much larger than the substrate area, and additionally generated grain boundaries, interface coupling and interface strain modulation.
Currently, films with vertically aligned nanostructures are predominantly two-phase composite films. Such vertically aligned nanostructures can typically be induced in self-assembled two-phase nanocomposite films due to the large lattice mismatch between the two phases and between each phase and the substrate. The second phase of the two-phase composite film is typically a binary or ternary metal oxide, such as ZnO, MgO, V2O3、Sm2O3、CeO2、NiO、CoFe2O4、NiFe2O4、BiFeO3、BaZrO3And the like. Enhanced physical properties and diverse functionalities including interface-induced high temperature superconductivity, significantly enhanced low field magnetoresistance, strain enhanced ferroelectricity, magnetoelectricity, multiferroics, and novel dielectric coupling and magneto-optical coupling effects, etc. can be obtained through strong coupling and interface and grain boundary effects between the two phases. However, so far, a single-phase thin film of a complex oxide having vertically aligned nanostructures has been rarely reported.
The synthesis of vertically aligned nanostructures is a very complex technique. For single-phase thin films, it is difficult to obtain the desired growth of vertically aligned nanostructures by merely controlling the lattice mismatch between the substrate and the thin film. In order to achieve the desired vertical alignment of the nanostructures, in addition to the lattice strain, thermodynamic and kinetic parameters, such as substrate temperature, oxygen pressure, composition, distance dimensions, growth rate, etc., need to be carefully adjusted, which is considered a very sophisticated technique. Perovskite manganese oxides have fascinating physical phenomena such as giant magnetoresistance, phase separation, large spin polarization, magnetic anisotropy and the like, thereby promoting the expectation of people on the development of spintronics. The intrinsic giant magnetoresistance effect of perovskite manganese oxides typically requires a high magnetic field of several tesla to trigger and is limited to a narrow temperature range, which hinders practical applications such as high density magnetic storage devices or magnetic head sensors, which often need to operate at low magnetic fields and wide temperature ranges. Therefore, the extrinsic low field magnetoresistance effect in perovskite manganese oxides is of greater concern. This external induced low field magnetoresistance effect can achieve high magnetoresistance at low magnetic fields (less than 1T) and over a wide temperature range. Achieving this low field magnetoresistance effect depends on the control of the microstructure, such as interfaces, grain and phase boundaries, and spin-polarized tunneling junctions.
The invention adopts a pulse laser deposition method to deposit a film, and simultaneously, in the deposition process, the microstructure of the film is adjusted by applying strong magnetic fields with different strengths, so as to prepare the double-layer perovskite manganese oxide single-phase film material which has vertical magnetic anisotropy, is adjustable and can work in a wide working temperature range and has a low field magnetoresistance effect.
Disclosure of Invention
The invention designs a vertically-arranged double-layer perovskite manganese oxide single-phase thin film material which has obvious vertical magnetic anisotropy, is adjustable, has a wide working temperature range and has a low field magnetoresistance effect.
The invention provides a preparation method for realizing an adjustable vertically-arranged nano-structure double-layer perovskite lanthanum calcium manganese oxygen single-phase thin film material.
The technical scheme designed by the invention is as follows:
the perovskite lanthanum calcium manganese oxygen single-phase film material is a film formed from lanthanum, calcium, manganese and oxygen elements.
The film is of the formula La1-xCaxMnO3Perovskite single-phase thin filmIn the chemical formula, La is lanthanum, Ca is calcium, Mn is manganese, and O is oxygen. x is an element component, and x is more than 0.35 and less than or equal to 1.
The double-layer perovskite structure is composed of two layers: a first layer of thin planar thin film structure grown continuously along the substrate and having a thickness of 0-40 nm; the second layer continues to grow epitaxially along the continuous planar film. At this time, the second layer has vertically aligned nanostructures. The structure grows up to the top of the film. The overall film thickness is related to the deposition time of the film, and the thickness can reach the micron order.
The preparation method comprises the following steps:
step 1, weighing lanthanum oxide, calcium oxide and manganese oxide according to the molar ratio of lanthanum, calcium, manganese and oxygen, uniformly grinding the lanthanum oxide, the calcium oxide and the manganese oxide through an agate pot, sintering the lanthanum oxide, the calcium oxide and the manganese oxide for multiple times at the high temperature of 1100-1400 ℃ to form lanthanum-calcium-manganese-oxygen powder, and finally sintering the lanthanum-calcium-manganese-oxygen target material through a die pressing sheet at the high temperature of 1100-1400 ℃;
step 2, firstly, installing the substrate and the lanthanum-calcium-manganese-oxygen target material prepared in S1 in a pulse laser deposition system, and then vacuumizing a cavity of the pulse laser deposition system through a molecular pump; before preparing the film, heating the substrate to 680 ℃, then applying a strong magnetic field which is more than or equal to 5T by using a superconducting magnet and is vertical to the plane of the substrate, and keeping the vacuum cavity of the pulse laser deposition system at the oxygen pressure of 0.35 mbar; when the magnetic field intensity meets the requirement, a KrF excimer laser in a pulse laser deposition system emits pulse laser to deposit a film, the wavelength of the pulse laser is 248 nm, the energy is 200 mJ, the repetition frequency is 5 Hz, and the deposition time is 30 minutes; after the deposition is finished, the film is subjected to in-situ heat treatment for 20 minutes under the conditions of the same magnetic field, substrate temperature and oxygen pressure as those in the deposition process.
The preparation method of the double-layer perovskite lanthanum calcium manganese oxygen single-phase thin film material is further optimized, and the high-intensity magnetic field is a steady-state high-intensity magnetic field (H is more than or equal to 5T); the substrate is a ceramic substrate or a semiconductor substrate. Wherein the ceramic substrate is a lanthanide aluminate substrate, a LaSatt (LSAT) or a strontium titanate substrate; the semiconductor substrate is a silicon substrate.
The application of the double-layer perovskite manganese oxide single-phase thin film material with the vertically-arranged nano structure in materials such as a perpendicular magnetic recording material, a magnetic memory or a magnetic head sensor and the like.
And respectively characterizing the prepared target product by using a scanning electron microscope and an X-ray diffractometer. From the results, it was found that the target product was an epitaxial thin film. Wherein the thickness of the film is more than 500 nm. Wherein, a continuous thin plane film is epitaxially grown from the substrate, the thickness is 0-40 nm, and a vertically arranged and epitaxially grown nano-pillar film is arranged on the plane film. The diameter of the nano-column is about 10-60 nm. The content and the components of each element in the film are the same as those of the target material. Secondly, the magnetic properties (SQUID) and the transport properties (PPMS) are respectively used for measuring the prepared target product, and the results show that the double-layer perovskite manganese oxide single-phase thin film with the vertically-arranged nano structure has the obvious characteristic of vertical magnetic anisotropy, and meanwhile, the transport results show that the low-field magnetic resistance of the thin film is up to 45% under the conditions that the temperature is 150K and the measuring magnetic field is 1T. Meanwhile, in the temperature range of 127-200K, the low-field magnetoresistance value is more than 25 percent. Thirdly, the preparation method has the characteristics that the stoichiometric ratio in the target product can be accurately controlled, the process is simple and easy to master, the required equipment is few, the preparation cost is low, and the large-scale industrial production is facilitated.
Drawings
FIG. 1 is a graph showing the results of scanning electron microscopy of the target product obtained in example 1.
FIG. 2 is a schematic diagram showing the microstructure evolution of a double-layer perovskite manganese oxide single-phase thin film with the increase of an applied magnetic field in the preparation process.
Fig. 3 is a graph of the X-ray diffraction (XRD) characterization results of the target product obtained in example 1.
FIG. 4 is a graph of the results of the magnetic test of the target product obtained in example 1.
FIG. 5 is a graph showing the results of the characterization of the target product obtained in example 1 using a transport measurement system.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
First commercially available or prepared by conventional methods:
lanthanum oxide, calcium oxide; manganese oxide or trimanganese tetroxide; a ceramic-based substrate or a semiconductor substrate as a substrate. Wherein the ceramic substrate is a LaSatt (LSAT) substrate, a lanthanum aluminate substrate or a strontium titanate substrate, and the semiconductor substrate is a silicon wafer.
< example 1>
The preparation method comprises the following specific steps:
s1, La according to formula1-xCaxMnO3X =0.5 is selected, i.e. the chemical formula of the material is La0.5Ca0.5MnO3Lanthanum oxide, calcium oxide and manganese oxide are respectively weighed according to the molar ratio of lanthanum, calcium and manganese, then uniformly ground by using an agate bowl, and then sintered at high temperature for multiple times to form lanthanum-calcium-manganese-oxygen powder. Finally, tabletting and sintering at high temperature through a die to form La0.5Ca0.5MnO3A target material.
S2 selection (LaAlO)3)0.3(Sr2AlTaO6)0.7(001)[LSAT(001)]A single crystal substrate. First, the substrate and La prepared in S1 were mixed0.5Ca0.5MnO3The target material is arranged in a pulse laser deposition system, and then the cavity is vacuumized. The substrate was first heated to 680 c before the thin film was prepared. Then, a superconducting magnet is used for applying a strong magnetic field of more than or equal to 5T perpendicular to the plane of the substrate. Furthermore, an oxygen pressure of 0.35 mbar is maintained in the vacuum chamber of the pulsed laser deposition system. And when the magnetic field intensity meets the requirement, emitting a pulse laser with the laser energy of 200 mJ and the repetition frequency of 5 Hz by an excimer laser to deposit the film for 30 minutes. After the deposition is finished, the film is subjected to in-situ heat treatment for 20 minutes under the conditions of the same magnetic field, substrate temperature and oxygen pressure as those in the deposition process.
And finally, performing microstructure characterization on the target product by using a scanning electron microscope, a TEM electron microscope and X-ray diffraction, wherein the microstructure characterization is respectively shown in fig. 1 and fig. 3. The magnetic property and the transport property of the target product were measured using a magnetic test platform (SQUID) and a transport test system (PPMS), respectively, as shown in fig. 4 and 5, respectively.
As can be seen from fig. 1, the target product obtained is a double-layer film with vertically aligned nano-structures, and the double-layer film structure is: a thin continuous planar film of thickness 0-40 nm adjacent to the substrate; the second layer is a vertically aligned layer of nano-pillars epitaxially grown on top of the continuous layer.
FIG. 2 is a schematic diagram of the evolution of the perovskite manganese oxide single-phase thin film from a planar film structure to a columnar structure and finally to a double-layer film structure as the magnetic field is applied to increase in the preparation process.
As can be seen from FIG. 3, the obtained objective product had high ductility.
As can be seen from fig. 4, the target product obtained under the condition of strong magnetic field has significant magnetic perpendicular anisotropy.
As can be seen from FIG. 5, the double-layered La having the vertically aligned nanostructure0.5Ca0.5MnO3The single phase thin film has an enhanced, tunable low field magnetoresistance effect, and the effect is suitable for a wide operating temperature range.
By selecting perovskite manganese oxide with different components, different ceramic substrates and different strong magnetic fields, the above example 1 can be repeated to obtain the double-layer single-phase thin film with the vertical arrangement nanometer structure similar to that shown in the figure 1, and the thin film material also has obvious vertical magnetic anisotropy and has wide working temperature range and obviously enhanced low-field magnetoresistance effect as shown by the curves in the figures 4 and 5.
It is apparent that those skilled in the art can make various changes and modifications to the manganese oxide single-phase thin film material of the double-layer perovskite structure of the present invention and the preparation conditions without departing from the spirit and scope of the present invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.

Claims (5)

1. A double-layer perovskite manganese oxide single-phase thin film material with a vertically-arranged nano structure, which is grown on a substrate, is characterized in that the double-layer perovskite manganese oxide single-phase thin film materialThe chemical formula of the film material is La1-xCaxMnO3X is more than 0.35 and less than or equal to 1, the double-layer structure of the nano-structure comprises a continuous layer with the thickness of 0-40 nm and epitaxially grown along the substrate and a nano-column layer vertical to the continuous layer, and the nano-column layer epitaxially grows along the continuous layer.
2. The double-layer perovskite manganese oxide single-phase thin film material with the vertically aligned nano-structure as claimed in claim 1, wherein the substrate is a ceramic substrate or a semiconductor substrate; wherein the ceramic substrate is a lanthanide aluminate substrate, a LaSatt or a strontium titanate substrate, and the semiconductor substrate is a silicon substrate.
3. The single-phase thin film material of double-layer perovskite manganese oxide with vertically aligned nano-structures as claimed in claim 1, wherein the diameter of single nano-pillar in the nano-pillar layer is 10-60 nm.
4. The method for preparing the double-layer perovskite manganese oxide single-phase thin film material with the vertically aligned nano structure according to claim 1, which is characterized by comprising the following steps:
s1, weighing lanthanum oxide, calcium oxide and manganese oxide according to the molar ratio of lanthanum to calcium to manganese to oxygen, uniformly grinding the lanthanum oxide, the calcium oxide and the manganese oxide through an agate pot, performing multiple high-temperature sintering to form lanthanum-calcium-manganese-oxygen powder, and finally performing high-temperature sintering through a die to prepare the lanthanum-calcium-manganese-oxygen target material; wherein the temperature of the high-temperature sintering is controlled at 1100-1400 ℃;
s2, growing a single-phase film on the substrate: firstly, a substrate and a lanthanum-calcium-manganese-oxygen target material prepared in S1 are installed in a pulse laser deposition system, and then a cavity of the pulse laser deposition system is vacuumized through a molecular pump; before preparing the film, heating the substrate to 680 ℃, then applying a strong magnetic field which is more than or equal to 5T by using a superconducting magnet and is vertical to the plane of the substrate, and keeping the vacuum cavity of the pulse laser deposition system at the oxygen pressure of 0.35 mbar; when the magnetic field intensity meets the requirement, a KrF excimer laser in a pulse laser deposition system emits pulse laser to deposit a film, the wavelength of the pulse laser is 248 nm, the energy is 200 mJ, the repetition frequency is 5 Hz, and the deposition time is 30 minutes; after the deposition is finished, carrying out in-situ heat treatment on the film for 20 minutes under the conditions of the same magnetic field, substrate temperature and oxygen pressure in the deposition process, thus obtaining the double-layer perovskite manganese oxide single-phase film material.
5. The use of the double-layer perovskite manganese oxide single-phase thin film material with the vertically aligned nano-structure according to claim 1 in a perpendicular magnetic recording material, a magnetic memory or a magnetic head sensor.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114592237A (en) * 2022-03-11 2022-06-07 淮北师范大学 Preparation method of epitaxial film

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